Pharmacogn J. 2019; 11(5):894-900.
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Characterization Sodium Carboxymethyl Cellulose from Alpha
Cellulose Betung Bamboo (Dendrocalamus asper)
Herman Suryadi*, Sutriyo, Ghina Fauziah
Herman Suryadi*, Sutriyo,
Ghina Fauziah
Faculty of Pharmacy, Universitas Indonesia,
Depok, INDONESIA.
Correspondence
Herman Suryadi
Faculty of Pharmacy, Universitas
Indonesia, Depok, INDONESIA.
Email: hsuryadi@farmasi.ui.ac.id
History
• Submission Date: 08-02-2019;
• Review completed: 12-04-2019;
• Accepted Date: 24-05-2019.
DOI : 10.5530/pj.2019.11.143
Article Available online
http://www.phcogj.com/v11/i5
Copyright
© 2019 Phcogj.Com. This is an open-
access article distributed under the terms
of the Creative Commons Attribution 4.0
International license.
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894
Original Article
ABSTRACT
Objective: Sodium carboxymethylcellulose (Na-CMC) is one of pharmaceutical excipients
that can be used to increase viscosity in topical, oral and parenteral pharmaceutical
formulation, beside that it can also be used as binder and disintegrant in tablet formulation.
Betung bamboo is one of natural material that contains high concentration of holocellulose
for about 83.80%. The purpose of this study was to characterize Na-CMC obtained through
alkalization and carboxymethylation reaction. Methods: Alkalization was carried out using 25%
sodium hydroxide and 1.7% sodium tetraborate. Carboxymethylation was done with sodium
monochloroacetate to alpha cellulose ratio 1.3 : 1. Product was identified by FTIR and further
characterized by XRD, SEM, DS value and pH. Result: The product was white colour powder
which has similarities of its infrared spectrum to reference. Other characteristics that showed
similarities to reference was degree of substitution 0.7073, pH 7.61, average of particle
size distribution 71.54 μm, moisture content 5.88%, sulfated ash content 32.64% and loss
on drying 9.85%. Conclusion: Based on the comparison of X-ray diffraction, there is similarity
between reference and product (Na-CMC) from betung bamboo. However, there were differences
in melting temperature, viscosity and morphological analysis with SEM to reference.
Key words: Betung bamboo, Cellulose, Sodium carboxymethylcellulose, Alkalization,
Carboxymethylation, Characterization.
INTRODUCTION carboxymethyl cellulose is synthesized through
two stages, alkalization and carboxymethylation.
Sodium carboxymethyl cellulose is used in oral and Alkalization was carried out using sodium
topical dosage formulations in pharmaceutical field. hydroxide that produces more reactive alkaline
Sodium carboxymethyl cellulose can also be used cellulose. Whereas in carboxymethylation, sodium
as binder and disintegrant in tablet formulation, monochloroacetate is used to produces sodium
increase viscosity and emulsifying agent.1 carboxymethyl cellulose.
In Indonesia, sodium carboxymethyl cellulose Previous research that conducted by Koh (2013)
that used in pharmaceutical industry is imported showed that 25% sodium hydroxide produces
from another country, it can cause drug prices sodium carboxymethyl cellulose with the highest
rise. Whereas, Indonesia has many natural sources degree of substitution (0,6047).4 But, in this research
of cellulose that can be used to produce sodium the pharmaceutical degree of substition (0, 7 – 1, 2)
carboxymethyl cellulose. was not fulfilled, therefore it is necessary to modify
Cellulose is the basic structure of plant cells that the method for preparing pharmaceutical sodium
made by living organisms. The most common carboxymethyl cellulose.
source of cellulose in the pharmaceutical field In this study, alpha cellulose will be obtained
is wood which has cellulose content of 40-50%.2 from isolation process and after that it will be
However, the use of wood as source of cellulose is used to produce sodium carboxymethyl cellulose.
considered less effective because wood is often used Furthermore, identification and characterization
as household raw material and has long growing will be performed by comparing the product with
time, therefore it is necessary to find another source sodium carboxymethyl standard.
of cellulose that has short growing time. Bamboo
has very short growing time. Bamboo can be MATERIALS AND METHODS
harvested within 4 years after planting, it is shorter
than wood that can be harvested in 8-20 years.3 Materials
Betung bamboo (Dendrocalamus asper) contains Betung bamboo powder that is used in this study was
83.80% holocellulose, 30.20% lignin, 4.63% ash, obtained from Balai Penelitian Tanaman Rempah
3.51% silica and extractive substances.3 Cellulose dan Obat (Balitro), Bogor.
of betung bamboo can be obtained from extraction
with organic solvent and isolation with alkaline
Tools and instruments
solution that produces alpha cellulose. Alpha The tools and instruments used in this study were
cellulose that obtained is used as a material for infrared spectrophotometry (FTIR-8400S Shimadzu,
produces sodium carboxymethyl cellulose. Sodium Japan), Differential Scanning Calorimetry
Cite this article: Suryadi H, Sutriyo, Fauziah G. Characterization Sodium Carboxymethyl Cellulose
from Alpha Cellulose Betung Bamboo (Dendrocalamus asper). Pharmacog J. 2019;11(5):894-900.
Pharmacognosy Journal, Vol 11, Issue 5, Sep-Oct, 2019
 Suryadi H, et al.: Characterization Sodium Carboxymethyl Cellulose from Alpha Cellulose Betung Bamboo (Dendrocalamus asper)
(PerkinElmer, USA), analytical balance (Sartorius, Germany), Bulk
density tester (BDT M4-005/04, Indonesia), pH meter (Eutech,
Singapore), furnace (Cole-Parmer, USA), Hot plate and stirrer (IKA
Tipe Hs-7, Germany), Particle Size Analyzer (CILAS 1190, France),
Scanning Electron Microscope (QUANTA 650, USA), X-Ray
Diffractogram (XRD Panalytical X’Pert Pro MPDb, Europe), Moisture
Content (ADAM AMB50, USA), Viscometer (Cole-Parmer, USA),
sintered funnel (Pyrex, Germany), filter paper (Whattman, Germany),
aluminium foil (Total Wrap, Indonesia), crucible (RRC, China), oven
(Heraeus, Germany), desiccator (Duran, Germany), burette (Pyrex,
Germany) and other glass wares commonly used in laboratories.
Chemicals
Chemicals used in this study were n-hexane (Merck, Germany),
ethanol 96% (Merck, Germany), nitric acid (Merck, Germany), sodium
hydroxide (Merck, Germany), sodium sulfite (Merck, Germany),
sodium nitrite (Merck, Germany), sodium hypochlorite (Merck,
Germany), sodium monochloroacetate (Merck, Germany), sodium
tetraborate (Merck, Germany), isopropyl alcohol (Merck, Germany),
potassium bromide (Merck, Germany), glacial acetic acid (Merck,
Germany), methanol (Merck, Germany), sulfuric acid (Merck,
Germany), hydrochloric acid (Merck, Germany), methyl red (Merck,
Germany), phenolphthalein (Merck, Germany), alpha naphthol
(Merck, Germany), anhydrous sodium carbonate (Merck, Germany),
potassium biphthalate (Merck, Germany), aquadestilata (Brataco,
Indonesia) and sodium carboxymethyl cellulose standard (Merck,
Germany) as reference.
METHODS
Extraction of Betung bamboo powder
The extraction process was done using the method of Kharismi.5 Before
the extraction, betung bamboo (Dendrocalamus asper) powder was
washed using water and was dried in 60°C oven for about 8 h. The
extarction process was carried out using maceration method with 2 L
of n-hexane-ethanol (2:1) as solvent for about 24 h. The residue from
filtering process was dried in room temperature for 24 h.
Isolation of Alpha cellulose from betung bamboo
The isolation of alpha cellulose from betung bamboo method of
Suryadi, Sutriyo, Sari and Rosikhoh was used.6 A 200 g of betung
bamboo powder was mixed in 2.67 L 3.5% nitric acid (contain 26.7 mg
sodium nitrite). The mixture was heated on hotplate at 90°C for 2 h.
After that the mixture was filtered and the residue was washed with
aquadestilata. It was digested with 2 L solution containing 2% w/v each
of sodium hydoxide and sodium sulfite at temperature of 50°C for 1
h. Again, it was washed, filtered and bleached with 1.34 L 1:1 aqueous
dilution of 3.5% w/v sodium hypochlorite at boiling temperature for
10 min. The washed and filtered material was next treated with 1.33
L 17.5% w/v sodium hydoxide at 80°C for 30 min. The resulting alpha
cellulose was washed thoroughly with aquadestilata and filtered. The
product was dried in 60°C oven for about 3 h.
Preparation of sodium carboxymethyl cellulose
The method of Koh with slight modification was used.4 First of all,
20 g of cellulose powder from betung bamboo was weight and added
to 600 mL isopropyl alcohol with continuous stirring. Then, 67 mL
of 25% sodium hydroxide (contain 1,7% sodium tetraborate) was
added dropwise into the mixture and further stirred for an h at room
temperature. The carboxymethylation was started when 26 g of sodium
monochloroacetate was added with continuous stirring for another 1.5
h. The mixture was covered with aluminium foil and placed on hotplate
at 55°C for 3 h. The slurry was subsequently soaked in 225 mL methanol.
It was neutralized with glacial acetic acid to pH 7 and than filtered
Pharmacognosy Journal, Vol 11, Issue 5, Sep-Oct, 2019
using sintered funnel. The final product was washed for three times
by soaking in ethanol 80% for 10 min and than it was washed again
with methanol for the last time. The obtained sodium carboxymethyl
cellulose from betung bamboo was filtered and dried at 55°C.
Identification and characterization
Infrared spectrum
Infrared spectra of sodium carboxymethyl cellulose was recorded
with FTIR-8400S Shimadzu. Pellets was made by using ± 1 mg sample
and ± 99 mg potassium bromide. Transmission was measured at the
wavelength number range of 4000 – 400 cm-1.
X-Ray diffraction (XRD)
XRD analysis was performed to see the crystalline and amorphous form
of sodium carboxymethyl cellulose. Sodium carboxymethyl cellulose
was analyzed using X-Ray Diffractogram Panalytical X’Pert Pro MPDb.
Scanning Electron Microscopy (SEM)
The morphological structure of sodium carboxymethyl cellulose was
analyzed using QUANTA 650 Scanning Electron Microscope.
Organoleptic examination
The characteristics of product (shape, color, taste and smell) was
compared with sodium carboxymethyl cellulose standard.
Qualitative analysis
1 g of sodium carboxymethyl cellulose was added in 50 mL aquadestilata
and stirred until the mixture homogeneous. 1 mL of solution was taken
and mixed with 1 mL aquadestilata, after that 5 drop of alpha naphthol
was added and than 2 mL sulfuric acid was added slowly. The reaction
shows positive result when purple color is formed.7
Melting temperature
10 mg of carboxymethyl cellulose was weighted and analyzed using
PerkinElmer Differential Scanning Calorimetry using heat from 40°C
to 900°C with heat flow 20°C/min.
Degree of substitution
1 g of dry sodium carboxymethyl cellulose was stirred in 20 mL ethanol
96% for 5 min. Than 5 mL of 2 M nitric acid was added, after that the
mixture was boiled. The solution was removed from the hotplate and
further stirred for 10 min. The mixture was separated into two parts,
which was solid and liquid phase. The liquid phase was removed and
the solid phase was washed with 10 mL of 80% ethanol at 60°C for 5
times. Lastly, the precipitate was dried at 100°C for 3 h.
The product was weighed and inserted to 250 mL erlenmeyer, 100 mL
of aquadestilata was added and stirred. Then 25 mL of 0.3 M sodium
hydroxide was added and heated to boil for 15 min. After the product
dissolved, the mixture was titrated with 0.3 M hydrochloric acid.
Phenolphtalein was added to observe the color change from dark pink
to colorless. The titration was repeated twice and the average volume of
hydrochloric acid used was recorded.4
Where:
Vo = mL of hydrochloric acid used to titrate blank,
Vn = mL of hydrochloric acid used to titrate samples,
M = molar concentration of hydrochloric acid used,
895
 Suryadi H, et al.: Characterization Sodium Carboxymethyl Cellulose from Alpha Cellulose Betung Bamboo (Dendrocalamus asper)

M = sample amount (g) Viscosity

162 g/mol is the molar mass of the anhydroglucopyranose unit (AGU)
and 59 g/mol is the molar mass of -CH2COOH
Degree of acidity (pH)
1 g of sodium carboxymethyl cellulose was added in 100 mL
aquadestilata and heated at 70°C until it dissolved. Degree of acidity of
solution was measured by Eutech pH meter.8
Analysis of particle size and particle size distribution
0.1 g of sodium carboxymethyl cellulose was weighted and dissolved in
10 mL destilled water. It was analyzed using CILAS 1190 particle size
analyzer.
Water content analysis
1 g of sodium carboxymethyl cellilose was weighted and analyzed using
ADAM AMB50 moisture content analyzer.
Sulfated ash content analysis
First of all, the crucible was burned in 600°C furnance for 30 min and
cooled in desiccator, after that the crucible was weighed until constant
weight. 1 g of sodium carboxymethyl cellulose was added to the crucible.
The crucible was burned and cooled in desiccator for 30 min. After that,
the residue was moistened with 1 mL aquadestilata and 1 mL sulfuric
acid. The mixture was heated gently until white fumes were no longer
evolved and ignited in the furnance until all black particles disappear.
The crucible was cooled in desiccator, few drop of aquadestilata-
sulfuric acid (1:1) was added and again heated. The ignition was carried
as before, cooled and then weighed. This was repeated until the sample
reached a constant weight.9
Loss on drying
1 g of sodium carboxymethyl cellulose was weighed and placed into
crucible. It was dried in oven at 105°C until the sample reached a
constant weight.9
Particle density
Bulk density and tapped density of sodium carboxymethyl cellulose
was measured using BDT M4-005/04 bulk density tester.
1 g of sodium carboxymethyl cellulose was weighed and dissolved in
100 mL aquadestilata. The viscosity of solution was measured using
Cole-Parmer Viscometer.
RESULT AND DISCUSSION
Isolation of alpha cellulose from betung bamboo
The isolation of alpha cellulose divided into three main processes. First
is the delignification. It was done using 3.5% nitric acid and the mixture
of 2% sodium hydroxide – 2% sodium sulfite (1:1). Second, bleaching
process using 10% sodium hydroxide – water (1:1) and the last was
dehemicellulose using 17.5% sodium hydroxide. The use of 17.5%
NaOH was intended to separate alpha cellulose fraction (insoluble)
from the soluble fraction (beta and gamma),2 this process was done
to obtain alpha cellulose that can be used to produce carboxymethyl
cellulose (Table 1).
Preparation of sodium carboxymethyl cellulose
Preparation of sodium carboxymethyl cellulose is divided into two
processes, alkalization and carboxymethylation. Alkalization was
carried out using 25% sodium hydroxide and 1.7% sodium tetraborate
with isopropyl alcohol as reaction medium. NaOH is used for convert
cellulose to alkali cellulose which is more reactive. Alkali brings about
the swelling of native cellulose fiber, which cause modifications of
crystallinity of cellulose structure and increased the accessibility of
carboxymethyl group to cellulose structure.10 Sodium tetraborate
was added to increase the quality of solution, which can also increase
the degree of substitution of the product.11 Carboxymethylation was
done with sodium monochloroacetate to alpha cellulose ratio 1.3:1.
Furthermore, the suspension was neutralized with glacial acetic acid
to pH 7. After that the suspension was washed using 80% ethanol and
methanol to eliminate the other impurities.4
From Table 2, the yield of Na-CMC is approximately ranging from
95.36% until 108.76%. The reason as why the yield can larger than the
raw material it self (cellulose) is due to the addition of monochloroacetic
acid during carboxymethylation.12

Table 1: Yield of cellulose from betung bamboo.

Mass of betung bamboo Mass of alpha cellulose Yield of alpha cellulose
200.77 gram 58.30 gram 29.04%
200.27 gram 53.90 gram 26.91%

Table 2: Yield of sodium carboxymethyl cellulose from alpha cellulose betung bamboo.
Mass of sodium
Mass of cellulose carboxymethyl cellulose Yield of Na-CMC
(Na-CMC)
20.0081 grams 19.0805 grams 95.36%
20.0175 grams 19.7198 grams 98.51%
20.0080 grams 21.7605 grams 108.76%

Table 3: Wavenumber of functional groups of avicel pH 101 and alpha cellulose from betung bamboo.
Wavenumber (cm-1)
Functional groups Alpha cellulose
Avicel pH 101
betung bamboo
OH 3338 3325
CH stretching 2899 2895
CH2 1429 1421
C-O-C glycosidic 1155 1153
C-OH 1047 1060

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 Suryadi H, et al.: Characterization Sodium Carboxymethyl Cellulose from Alpha Cellulose Betung Bamboo (Dendrocalamus asper)
Identification and characterization
Functional groups that showed in infrared spectra of alpha cellulose
consists of OH group at wavenumber 3650-3200 cm-1, CH stetching at
3000-2850 cm-1, CH2 at 1465 cm-1, C-OH bond at 1000-1260 cm-1 and
C-O-C glycosidic at 1200-980 cm-1 (Figure 1 and Table 3).13-15
Carboxyl groups and its salt show two peaks at the wavenumber about
1600 – 1640 cm-1 and 1400 – 1450 cm-1 which indicates the presence
of carboxymethyl substituent. The band around 1421 – 1425 cm-1 and
1325 cm-1 are assignedto CH2 scissoring and OH bending vibration
(Figure 2 and Table 4).15
XRD analysis was conducted to see the shape of the crystal sample
compared to reference, Na-CMC standard. The X-ray diffractogram
of crystalline polymers produce sharp peak, while the amorphous
polymers tend to produce a widened or blund peak.6 Diffractogram of
Na-CMC from alpha cellulose betung bamboo showed the similarity
with diffractogram reference. In Na-CMC standard there is a typical
pattern of diffractogram, on 2θ value of 19.985 contained a sharp peak
that shows the nature of the crystalline and on 2θ value of 36.8801 the
blunt and widened peak or valley shows amorphous nature (Figure
3a). While Na-CMC from alpha cellulose betung bamboo indicated 2θ
value of 19.7343 contained a sharp peak and on 2θ value of 35.4429
contained the blunt and widened peak (Figure 3b).
Figure 1: Infrared spectrum of avicel pH 101 (red) and alpha cellulose from betung bamboo (black).
Table 4: Wavenumber of functional groups of Na-CMC standard and Na-CMC from alpha cellulose betung bamboo.
Functional groups
Na-CMC standard
OH 3607
CH stretching 2877
C=O carboxyl 1678
CH2 1431
OH binding vibration 1325
C-O-C glycosidic 1153
C-OH 1064
Pharmacognosy Journal, Vol 11, Issue 5, Sep-Oct, 2019
Analysis with scanning electron microscope showed Na-CMC standard
and Na-CMC from alpha cellulose from betung bamboo have different
morphological structure. The standard has long-shape with relatively
smooth surface (Figure 4), however Na-CMC from alpha cellulose
betung bamboo has round-shape with relatively rough surface (Figure
5). This difference can occur due to the use of alpha cellulose (raw
materials) from different sources (Table 5).16
The characterization processes of Na-CMC from alpha cellulose betung
bamboo which was compared with reference showed the similarity.
However, the melting temperature of the product was higher than
reference, it showed that there were still impurities in the product.
Particle density of the product and the reference also showed the
differences, the product has higher particle density because the mass of
the product is heavier than standard reference. Moreover the viscosity
of the product and the reference showed a huge difference, the product
could be categorized as medium viscosity Na-CMC, while the reference
was as medium viscosity grade Na-CMC. That can occur due to the use
of alpha cellulose from different sources.17
CONCLUSION
The product showed similarity of the characteristics to the reference on
infrared spectra, XRD diffractogram, organoleptic analysis, qualitative
Wavenumber (cm-1)
Na-CMC from alpha
cellulose
betung bamboo
3618
2879
1678
1421
1325
1126
1020
897
 Suryadi H, et al.: Characterization Sodium Carboxymethyl Cellulose from Alpha Cellulose Betung Bamboo (Dendrocalamus asper)

Figure 2: Infrared spectrum of Na-CMC standard (red) and Na-CMC from alpha cellulose betung bamboo (black).

1100 1000
Standar
Na-CMC CMC
standard Standar
Na-CMC from alphaCMC Ghina
cellulose
1000 900
betung bamboo
900 800
Intensity (Count)
Intensity (Count)

800
700
700
600
600
500
500
400
400
300
300
200
200

100 100
10 20 30 40 50 60 70 80 90 100 10 20 30 40 50 60 70 80 90 100
2θ 2θ

Figure 3: X-ray diffractogram of Na-CMC standard and Na-CMC from alpha cellulose betung bamboo.

Table 5: The result of characterization Na-CMC from alpha cellulose betung bamboo compared with Na-CMC standard.
Na-CMC from alpha cellulose
Characterization Na-CMC standard
betung bamboo
Organoleptic White powder, odorless and tasteless White powder, odorless and tasteless
Positive Positive
Qualitative analysis
(purple color was formed) (purple color was formed)
Melting temperature 230.10°C 255.30°C
Degree of substitution 0.7433 0.7073
Degree of acidity (pH) 6.93 7.61
Average of particle size distribution 55.13 μm 71.54 μm
Water content 9.86% 5.88%
Sulfated ash content 31.29% 32.64%
Loss on drying 10.17% 9.85%
Particle density
Bulk density 0.33 g/cm3 0.42 g/cm3
Tapped density 0.50 g/cm3 0.64 g/cm3
Viscosity 3527.7 Cp 20.8 Cp

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 Suryadi H, et al.: Characterization Sodium Carboxymethyl Cellulose from Alpha Cellulose Betung Bamboo (Dendrocalamus asper)
Figure 4: The result of SEM Na-CMC standard.
Figure 5: The result of SEM Na-CMC from alpha cellulose betung bamboo.
analysis, degree of substitution, degree of acidity (pH), average of
particle size distribution, water content, sulfated ash content and loss
on drying. However, there were differences in melting temperature,
viscosity and morphological analysis with SEM to reference.
SUGGESTION
It is necessary to do the optimization of the alpha cellulose isolation
process which produce higher yield of alpha cellulose. Beside that, it is
also necessary to reasearch the degree of polimerization and molecular
weight to show the correlation with the viscosity of the product.
ACKNOWLEDGEMENT
This study was supported by Hibah Publikasi Internasional Terindeks
Untuk Tugas Akhir Mahasiswa UI (PITTA) 2018 by Universitas
Indonesia. We thank PITTA 2018 for providing the fund that used in
the study.
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Cite this article: Suryadi H, Sutriyo, Fauziah G. Characterization Sodium Carboxymethyl Cellulose from Alpha Cellulose Betung
Bamboo (Dendrocalamus asper). Pharmacog J. 2019;11(5):894-900.

900 Pharmacognosy Journal, Vol 11, Issue 5, Sep-Oct, 2019